Instituto de Cerámica y Vidrio (CSIC), Campus de Cantoblanco, Calle Kelsen 5, 28049 Madrid, Spain.
Talanta. 2010 Apr 15;81(1-2):301-8. doi: 10.1016/j.talanta.2009.11.072. Epub 2009 Dec 16.
A systematic study on the influence of relative abundance of isotopes of elements in the coating (A(c)) and in the substrate (A(s)) on both shape of time-resolved signals and depth resolution (Delta z) was performed for depth profile analysis of metal coatings on metal substrates by ultraviolet (266 nm) nanosecond laser ablation inductively coupled plasma quadrupole mass spectrometry. Five coated samples with coating thicknesses of the same order of magnitude (20-30 microm) were tested: nickel coating on aluminium, chromium and copper, and steel coated with copper and zinc. A laser repetition rate of 1 Hz and a laser fluence of 21 J cm(-2) were used. Five different depth profile types were established, which showed a clear dependence on A(c)/A(s) ratio. In general, depth profiles obtained for ratios above 1-10 could not be used to determine Delta z. We found that Delta z increased non-linearly with A(c)/A(s) ratio. The best depth profile types, leading to highest depth resolution and reproducibility, were attained in all cases by using the isotopes with low/medium A(c) values and with the highest A(s) values. In these conditions, an improvement of up to 4 times in Delta z values was achieved. The average ablation rates were in the range from 0.55 microm pulse(-1) for copper coating on steel to 0.83 microm pulse(-1) for zinc coating on steel, and the Delta z values were between 2.74 microm for nickel coating on chromium and 5.91 microm for nickel coating on copper, with RSD values about 5-8%.
采用紫外(266nm)纳秒激光烧蚀电感耦合等离子体质谱法对金属基体上的金属涂层进行深度剖析时,系统研究了涂层(A(c))和基体(A(s))中元素同位素相对丰度对时间分辨信号形状和深度分辨率(Δz)的影响。测试了五个具有相同数量级(20-30μm)涂层厚度的涂层样品:镍涂层在铝、铬和铜上,钢涂层在铜和锌上。激光重复频率为 1Hz,激光能量密度为 21J/cm²。建立了五种不同的深度剖析类型,这些类型明显取决于 A(c)/A(s)比值。一般来说,比值高于 1-10 的深度剖析类型不能用于确定 Δz。我们发现 Δz 随 A(c)/A(s)比值呈非线性增加。在所有情况下,通过使用 A(c)值低/中等且 A(s)值最高的同位素,可以获得最佳的深度剖析类型,从而实现最高的深度分辨率和重现性。在这些条件下,Δz 值可提高 4 倍。平均烧蚀速率在钢上的铜涂层为 0.55μm/pulse 到钢上的锌涂层为 0.83μm/pulse 之间,Δz 值在铬上的镍涂层为 2.74μm 到铜上的镍涂层为 5.91μm 之间,RSD 值约为 5-8%。